CN109529793A - A kind of preparation method and application of magnetic hydrotalcite carried titanium dioxide composite material - Google Patents
A kind of preparation method and application of magnetic hydrotalcite carried titanium dioxide composite material Download PDFInfo
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- CN109529793A CN109529793A CN201811354137.1A CN201811354137A CN109529793A CN 109529793 A CN109529793 A CN 109529793A CN 201811354137 A CN201811354137 A CN 201811354137A CN 109529793 A CN109529793 A CN 109529793A
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- Prior art keywords
- composite material
- titanium dioxide
- flt
- preparation
- dioxide composite
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 44
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 44
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 44
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 33
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001179 sorption measurement Methods 0.000 claims abstract description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 7
- 238000000975 co-precipitation Methods 0.000 claims abstract description 7
- 229910000611 Zinc aluminium Inorganic materials 0.000 claims abstract description 6
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 31
- 230000015572 biosynthetic process Effects 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 11
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 1
- 239000011651 chromium Substances 0.000 abstract description 102
- 239000002114 nanocomposite Substances 0.000 abstract description 40
- 238000010521 absorption reaction Methods 0.000 abstract description 39
- 230000001699 photocatalysis Effects 0.000 abstract description 38
- 238000000034 method Methods 0.000 abstract description 20
- 238000007146 photocatalysis Methods 0.000 abstract description 18
- 230000008901 benefit Effects 0.000 abstract description 9
- 239000011701 zinc Substances 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 8
- 229910002651 NO3 Inorganic materials 0.000 abstract description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 231100000331 toxic Toxicity 0.000 abstract description 5
- 230000002588 toxic effect Effects 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- 229910052725 zinc Inorganic materials 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 229940056319 ferrosoferric oxide Drugs 0.000 abstract description 2
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 abstract description 2
- 239000004411 aluminium Substances 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 102100023593 Fibroblast growth factor receptor 1 Human genes 0.000 description 61
- 101000827746 Homo sapiens Fibroblast growth factor receptor 1 Proteins 0.000 description 61
- 102100033178 Vascular endothelial growth factor receptor 1 Human genes 0.000 description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 47
- 239000000463 material Substances 0.000 description 47
- 239000010936 titanium Substances 0.000 description 17
- 108010053096 Vascular Endothelial Growth Factor Receptor-1 Proteins 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 238000006722 reduction reaction Methods 0.000 description 10
- 238000010531 catalytic reduction reaction Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 101100381481 Caenorhabditis elegans baz-2 gene Proteins 0.000 description 2
- 229910017135 Fe—O Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 101100372762 Rattus norvegicus Flt1 gene Proteins 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 230000004069 differentiation Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 description 1
- 229910000604 Ferrochrome Inorganic materials 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 229910003088 Ti−O−Ti Inorganic materials 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/007—Mixed salts
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method and application of magnetic hydrotalcite carried titanium dioxide composite material, the composite material includes magnetic zinc-aluminum hydrotalcite and titanium dioxide, titanium dichloride load is on magnetic zinc-aluminum hydrotalcite, preparation method are as follows: using the nitrate and sodium hydroxide of zinc and aluminium, natrium carbonicum calcinatum, ferroso-ferric oxide and titanium dioxide as raw material, coprecipitation reaction is first carried out, hydrothermal crystallizing processing is then carried out；Magnetic hydrotalcite carried titanium dioxide composite material of the invention has many advantages, such as large specific surface area, large amount of adsorption, good to UV Absorption, it is a kind of nanocomposite that toxic Cr (VI) in water removal is gone by the method adsorbed and photocatalysis cooperates with, with nontoxic, low cost, the advantages that preparation method is simple, it can be widely applied for heavy metal chromium in adsorption photochemical catalysis reducing waste water, and reusing is preferable.
Description
Technical field
The present invention relates to a kind of adsorbent and ultraviolet light catalysts, and in particular to a kind of magnetic hydrotalcite carried titanium dioxide
The preparation method and application of composite material.
Background technique
Chromium is widely used in many industrial circles, such as plating, dyestuff, leather tanning, corrosion control and ferrochrome industry；With
Other common heavy metals such as lead, cadmium are different, and chromium is mainly present in water environment in the form of Cr (VI) and Cr (III)；Due to Cr
(VI) toxicity to environment and the mankind and mobility are above Cr (III), therefore generally select Cr (VI) being reduced to Cr (III)
As the effective ways for removing Cr (VI) in environment.
The method that Cr (VI) is removed from waste water is varied, mainly includes chemical precipitation, absorption, photo catalytic reduction, anti-
A variety of methods such as infiltration, electrochemical reduction, ion exchange, in these processes, absorption are a kind of cheap technologies, its advantage is that
It is easy to operate, at low cost；Common adsorbent have chemical fertilizer industry waste residue, modification of chitosan, iron oxide, calcining magnalium hydrotalcite,
Activated alumina and active carbon etc., wherein hydrotalcite is wide due to causing with biggish specific surface area and special structure
General concern.
Hydrotalcite is the fertile absorber of heavy metal in water removal, is that a kind of anionic quickly grown in recent years is viscous
Soil is a kind of lamellar compound with two dimension pattern plate structure, typical chemical general formula are as follows: [M1x 2+Mx 3+(OH)2]
[An-]x/n·yH2O, wherein M2+And M3+Divalent and trivalent metal cation respectively on laminate；An-It is interlayer anion；X is
M3+With (M2++M3+) molar ratio, usual range is from 0.17 to 0.33；Y is the number of interlayer hydrone；Hydrotalcite has wide
General chemical component, variable layer charge density, ion-exchange performance, reaction interlayer spaces, memory effect, flame retardant property, stream
Become the properties such as and colloidal property, although LDHs has stronger absorption property, its separative efficiency is lower.Meanwhile Magneto separate
Technology is taken seriously since additional magnetic is easily isolated.Although absorption method can greatly reduce pollution, adsorption effect cannot be shown
The validity for showing the removal of high density pollution object, does not meet the standard of the World Health Organization generally also；It is received currently with titanium correlation
Rice material (including TiO2And titanate) carry out the selection well that photocatalysis is removal Cr (VI).
Photocatalytic process is by TiO2Equal semiconductors are completed under ultraviolet light, TiO2Due to quantum size effect etc.
Excellent chemistry and optical property has very strong adsorption capacity in UV light region, higher photocatalytic activity is shown, in dirt
Contaminating improvement field has very big potentiality, is widely used in the degradation etc. of the photo catalytic reduction, organic matter of Cr (VI)；And
And TiO2Since its is nontoxic, chemical stability, photocatalytic activity and the advantages that low cost, be in advanced oxidation processes it is a kind of very
There is the semiconductor light-catalyst of application prospect；But TiO2There is light induced electrons and hole to height in the practical application of water process
The defect of recombination, limits TiO2Efficient application.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide it is a kind of it is novel by absorption and
The method of photocatalysis collaboration, removes large specific surface area, large amount of adsorption and the magnetic good to UV Absorption of toxic Cr (VI) in water removal
Property hydrotalcite carried titanium dioxide composite material, which has nontoxic a, low cost, and it is excellent that preparation method is simple etc.
Point.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material, which comprises the steps of:
The preparation of S1, magnetic hydrotalcite: Zn (NO will be contained3)2.6H2O、Al(NO3)3.9H2The mixed salt solution of O and
Contain NaOH, Na2CO3Mixed ammonium/alkali solutions be added drop-wise to Fe3O4Water slurry solution in carry out coprecipitation reaction, be centrifuged, collect
Solid formation cleans solid formation to neutrality with deionized water, dries to get magnetic hydrotalcite Fe is arrived3O4- LDH composite material, referred to as
FL composite material；
The preparation of S2, magnetic hydrotalcite carried titanium dioxide composite material: by TiO2PEG (200) are dissolved in, and weigh step
Magnetic hydrotalcite Fe made from S13O4- LDH composite material is added in PEG (200) solution, TiO2With Fe3O4- LDH composite material
Mass ratio is 1:1-10, and then ultrasound 20-40min, obtains slurries；
S3, above-mentioned slurries are subjected to hydrothermal crystallizing processing, after the reaction was completed, solid formation is collected in centrifugation, clear with deionized water
Solid formation is washed, it is dry, obtain Fe3O4-LDH-TiO2Class magnetic hydrotalcite catalyst, abbreviation FLT composite material.
In above-mentioned preparation method, it is preferred that press Fe in step S13O4And Al3+Molar ratio is (0.1~1): 1 ratio claims
Take paramagnetic nanoparticles Fe3O4, stirring under 60 DEG C of water bath conditions, Zn (NO will be contained3)2.6H2O、Al(NO3)3.9H2The mixing of O
Metal salt solution and contain NaOH, Na2CO3Mixed ammonium/alkali solutions, be added drop-wise to Fe3O4Water slurry solution in, and adjust reaction
The pH value of system is 9~10, carries out coprecipitation reaction.
In above-mentioned preparation method, it is preferred that weigh Zn (NO according to the ratio that zinc-aluminium molar ratio is 2: 1 in step S13)2.6H2O、Al(NO3)3.9H2O。
In above-mentioned preparation method, it is preferred that weigh Na according to the ratio that mass ratio is 9: 7 in step S12CO3With NaOH.
In above-mentioned preparation method, it is preferred that drying temperature is 40-60 DEG C in step S1.
In above-mentioned preparation method, it is preferred that further include that will obtain magnetic hydrotalcite Fe in step S13O4- LDH composite material
It sieves with 100 mesh sieve.
In above-mentioned preparation method, it is preferred that in step S3, the temperature of hydrothermal crystallizing processing is 80-100 DEG C, time 1-
2h。
In above-mentioned preparation method, it is preferred that in step S3, drying temperature is 60 DEG C.
The present invention also provides application of the FLT composite material made from above-mentioned preparation method in processing water in Cr (VI).
The present invention also provides the methods of Cr (VI) in application processing water, comprising the following steps: by the FLT catalyst
It is mixed with containing Cr (VI) waste water, adsorption photochemical catalysis reduction is carried out under illumination condition, complete the processing to Cr (VI) waste water.
Compared with the prior art, the advantages of the present invention are as follows:
(1) the present invention provides a kind of magnetic hydrotalcite carried titanium dioxide composite materials, including magnetic zinc-aluminum hydrotalcite
And titanium dioxide, wherein Fe3O4The combination of nano particle can be enhanced composite material and separate from aqueous solution and redisperse repetition benefit
Use performance；Titanium dichloride load improves the specific surface area of material in magnetic zinc-aluminum gavite, increases material adsorption energy
Power；The material has preferable catalytic performance under ultraviolet light, compensates for the low disadvantage of titanium dioxide ultraviolet utilization efficiency；It compares
In the material of other same types, FLT material of the invention have large amount of adsorption, large specific surface area, reusing it is good, to ultraviolet
The advantages that light absorption is good.
(2) the present invention provides a kind of preparation methods of magnetic hydrotalcite carried titanium dioxide composite material, with zinc and aluminium
Nitrate and sodium hydroxide, natrium carbonicum calcinatum, ferroso-ferric oxide and titanium dioxide be raw material, be prepared into using coprecipitation
It arrives；Compared to other prior arts, raw material sources of the invention are extensive and cheap, while normal in room temperature using coprecipitation
Pressure can carry out, and without high temperature and pressure and without the addition of toxic reagent, have low in cost, simple without special installation, operation
The advantages that folk prescription is just, preparation process is environmentally protective, convenient for large-scale production.
(3) the present invention also provides magnetic hydrotalcite carried titanium dioxide composite materials to administer toxic Cr (VI) in waste water
Using toxic Cr (VI) catalysis can be reduced to Cr (III) under ultraviolet light by FLT composite material of the invention, can not only be had
The Cr (VI) being adsorbed on material can also be effectively reduced to Cr (III) by effect absorption Cr (VI), single compared to other materials
Suction-operated, FLT of the invention can effectively adsorb pollutant and separate from aqueous solution, while FLT of the invention is repeated
Usability is preferable, and for 50mg/L Cr (VI), removal rate is 63.46% for the first time, right by 5 repetition adsoption catalysis processes
The removal rate of Cr (VI) is still up to 43.10%.
Detailed description of the invention
Fig. 1 is the preparation flow figure of magnetic hydrotalcite carried titanium dioxide composite material of the invention.
Fig. 2 is the mechanism schematic diagram that FLT removes Cr (VI).
Fig. 3 is Fe3O4、Fe3O4-LDH、TiO2With the FTIR spectrum (a) and XRD spectra (b) of FLT.
Fig. 4 is SEM (A), TEM (B, C), HRTEM (D) image of FLT-2.
Fig. 5 is the Elemental redistribution of FLT-2.
Fig. 6 is the EDS constituent content of FLT-2.
The high-resolution XPS spectrum (a), Fe 2p (b) and Ti 2p (c) spectrogram that Fig. 7 is FLT-2.
Fig. 8 is TiO2With the photocurrent response (a) and DRS absorption spectrum (b) of FLT composite material.
Fig. 9 is TiO2With the EIS analysis chart of FLT composite material.
Figure 10 is Fe3O4-LDH、TiO2, FLT absorption Cr (VI) reaction time (a), quasi- second-order kinetic equation (b), inhale
Attached thermoisopleth (c), langmuir equation (d) figure.
Figure 11 is Fe3O4- LDH, FLT are to photo catalytic reduction Cr (VI) effect (a) and reaction rate constant (b).
Figure 12 is Fe3O4-LDH、TiO2The collaboration of 50mg/L Cr (VI) (a) He 20mg/L Cr (VI) (b) are inhaled with FLT
Attached-photocatalysis.
Figure 13 is the experiment cycle-index that FLT-2 removes Cr (VI).
Figure 14 is FLT-2, AFLT-2 (after absorption), the infrared spectrogram of RFLT-2 (after catalysis reduction).
Figure 15 is the high-resolution of Fe 2p (a), Cr 2p (b), O 1s (c), Ti 2p (d) in FLT-2, AFLT-2, RFLT-2
XPS spectrum figure.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated；It should be understood that these embodiments are merely to illustrate the present invention
Rather than the claimed range of the limitation present invention；It will further be understood that read the content lectured of the present invention it
Afterwards, those skilled in the art can make various changes or modification to the present invention, and such equivalent forms are equally fallen within appended by the application
Claims limited range.
Embodiment 1
As shown in Figure 1, for a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material of the present invention, including such as
Lower step:
The preparation of S1, magnetic hydrotalcite:
Weigh 2.3g Fe3O4For ultrasonic disperse in 100mL distilled water, being placed in 60 DEG C of water-baths constantly stirring makes its dispersion
Uniformly, by 11.88g Zn (NO3)2·6H2O and 7.5g Al (NO3)3·9H2O, which is dissolved in, to be made into molar ratio in 250mL beaker and is
The solution of 2:1 is set to solution A, by 7.2g NaOH and 5.6g Na2CO3Be dissolved in solution formed in 250mL beaker be set to it is molten
Liquid B；Solution A and solution B are added drop-wise to Fe under 60 DEG C of water bath conditions3O4Dispersion solution in, and adjust solution pH be 9-
10, after the reaction was completed, centrifugation is collected solid formation, until cleaning solid formation to neutrality with deionized water, is dried under the conditions of 60 DEG C
It is dry, it sieves with 100 mesh sieve to get magnetic hydrotalcite Fe is arrived3O4- LDH composite material, abbreviation FL.
S2, synthesizing magnetic hydrotalcite carried titanium dioxide composite material
Scheme one: by 1.0g TiO2It is added in beaker after mixing with 60mL PEG (200), weighs 4.0g FL and add
It is added in mixture, then ultrasonic 30min pours into mixture in reaction kettle, heat 60min under the conditions of 95 DEG C；To material
After being cooled to room temperature, centrifugation collects solid formation, cleans solid formation with deionized water to remove excessive PEG (200), then exist
It is dried under the conditions of 60 DEG C, obtains Fe3O4-LDH-TiO2, abbreviation FLT, TiO in sample2Content is 20%, is named as FLT-2.
Scheme two: by 1.0g TiO2It is added in beaker after mixing with 60mL PEG (200), weighs 9g Fe3O4-
LDH composite material is added in mixture, then ultrasonic 30min pours into mixture in reaction kettle, heats under the conditions of 95 DEG C
60min；After material is cooled to room temperature, centrifugation collects solid formation, cleans solid formation with deionized water to remove excessive PEG
(200), it is then dried under the conditions of 60 DEG C, obtains Fe3O4-LDH-TiO2, TiO in sample2Content is 10%, is named as FLT-
1。
Scheme three: by 1.0g TiO2It is added in beaker after mixing with 60mL PEG (200), weighs 1g Fe3O4-
LDH composite material is added in mixture, then ultrasonic 30min pours into mixture in reaction kettle, heats under the conditions of 95 DEG C
60min；After material is cooled to room temperature, centrifugation collects solid formation, cleans solid formation with deionized water to remove excessive PEG
(200), it is then dried under the conditions of 60 DEG C, obtains Fe3O4-LDH-TiO2, TiO in sample2Content is 50%, is named as FLT-
5。
FT-IR is the important method for studying functional group's variation, therefore the present invention uses FT-IR to Fe3O4、TiO2、Fe3O4-
LDH, FLT-1, FLT-2, FLT-5 nanocomposite are characterized, as a result as shown in Fig. 3 (a), for Fe3O4-LDH、
FLT-1, FLT-2, FLT-5 nanocomposite, with 3300-3500cm-1Centered on Qiang Erkuan band and interlayer hydrone
The O-H stretching vibration of middle hydroxyl is related, 1366cm-1The peak value of left and right is attributable to CO3 2-With OH-The interaction of group, this says
It is bright that there are CO in LDHs3 2-Ion, 400~900cm-1Peak it is related with the stretching vibration of M-O and M-OH and bending vibration；
Fe3O4In 581cm-1Adsorption peak it is related with the vibration of Fe-O, 1632cm-1Peak be due in Fe3O4In synthesis process-
NH3、-NH2Or-NH planar stretches formation；For TiO2, in 400-800cm-1Low frequency region exists related to Ti-O-Ti
Absorption band；And for the composite material of above-mentioned different proportion synthesis, they have above-mentioned peak value.
Fig. 3 (b) is Fe3O4、TiO2、Fe3O4The XRD spectra of-LDH, FLT-1, FLT-2, FLT-5 nanocomposite,
The peak of FLT-2 is in 2 θ=11.7 °, and 23.6 °, 30.3 °, 34.7 °, 35.6 °, 39.2 °, 43.2 °, 46.9 °, 54.0 °, 56.9 °,
60.3 °, 61.7 ° and 62.8 °, respectively it is shown that Fe3(003) of O4-LDH, (006), (220), (012), (311),
(015), (400), (018), (442), (511), (110), (113), (440) crystal face characteristic peak；In 2 θ=25.5 °,
37.9 °, 48.1 °, 55.1 °, 62.8 °, 68.8 °, 70.4 ° and 75.1 ° be shown titanium dioxide (101), (004), (105),
(211), (204), (116), (220), (215) crystal face diffraction maximum；Without occurring significantly not in the XRD spectra of FLT-2
Pure diffraction maximum, this illustrates that nano material is highly purified；And FLT nanocomposite shows TiO2Phase and Fe3O4- LDH phase
Superposition, illustrate that FLT composite material synthesizes successfully；(003) plane included angle indicates that LDHs interfloor distance is larger；Such as (101) diffraction
Peak, (004) diffraction maximum and these roomy diffraction maximums of (200) diffraction maximum belong to TiO2Anatase；It can from Fig. 3 (b)
To find out, the material of above-mentioned different proportion synthesis includes above-mentioned all peaks；But peak strength is different, may have with different proportion
It closes, this also demonstrates TiO2And Fe3O4The crystal structure of-LDH is not influenced by additive amount.
The pattern of the FLT-2 nanocomposite prepared, crystal phase and composition are carried out by SEM, TEM and HRTEM
Characterization, as a result as shown in Figure 4；Fig. 4 (A) is the scanning electron microscope (SEM) photograph of FLT-2 nanocomposite, spherical Fe3O4, stratiform Zn-
Al-LDH and column TiO2It is interweaved, and spherical shape Fe3O4Uniform particle sizes；As the TEM image in Fig. 4 (B), Fig. 4 (C) also turns out
This point；The lattice fringe such as Fig. 4 (D) of FLT-2 in 0.2943,0.3507 and 0.2657nm is shown, is in close proximity to FLT-2
XRD spacing (2 θ=30.28 °, d=0.2949nm；2 θ=25.51 °, d=0.3490nm；2 θ=34.77 °, d=
0.2639nm)。
In order to study distribution of Al, Fe, O, Ti, Zn and S each element on FLT-2 nanocomposite, detailed characterizations
The Elemental redistribution of Al, Fe, O, Ti, Zn and S, as a result as shown in figure 5, EDS image as shown in fig. 6, by Fig. 5, Fig. 6 result it is found that
It include tested various elements on material；The above results illustrate that FLT-2 nanocomposite successfully synthesizes.
It is studied using surface composition and electronic structure of the XPS to FLT-2 nanocomposite, Fig. 7 (a) is FLT-
The XPS analysis spectrum of 2 nanocomposites；By result in Fig. 7 (a) it is found that Fe, Zn, Al, C, Ti and O are present in FLT-2 nanometers
In composite material；Two main peaks (Fig. 7 of Fe 2p, Fe 2p3/2 and Fe 2p1/2 can be observed at 708.8 and 722.3eV
(b)), illustrate Fe3O4It is present in nanocomposite；Fig. 7 (c) is the spectrum curve of Ti 2p1/2 and Ti 2p3/2 in sample,
Proof has Ti element, illustrates that there are TiO for FLT-2 nanocomposite catalyst surface2Particle.
Embodiment 2
In order to study TiO2, FLT-1, FLT-2, FLT-5 nanocomposite photocatalytic mechanism, the present invention use transient state
Photocurrent response and electrochemical impedance characteristic explain, as a result as shown in Fig. 8 (a) and Fig. 9；By Fig. 8 (a) it is found that FLT-
1, the transient photocurrents of FLT-2, FLT-5 are significantly greater than TiO2Material illustrates that the separative efficiency in light induced electron and hole obtains
It improves, to improve photocatalysis performance；As shown in Figure 9, the arc radius of the composite material of FLT-2 is minimum and FLT nanometers all
The arc radius of composite material is respectively less than TiO2Material illustrates that electronics is easier to transmit in FLT nanocomposite, this result
The photocatalysis performance for having convincingly demonstrated FLT nanocomposite is improved.
The present invention is also evaluated using optical property of the UV-vis diffusing reflection spectrum to sample, as a result such as Fig. 8 (b) institute
Show.TiO2There is strong absorption in the ultraviolet region as caused by electric charge transfer of the oxygen atom 2p track to Ti element three-dimensional space
Band；As shown in Fig. 8 (b), FLT under ultraviolet light with good absorption characteristic is shown under visible light, it is seen that the absorption under light
Reason may be related with the color of material itself, and by display in Fig. 8 (b), the absorption intensity of titanium dioxide is multiple better than FLT nanometers
Condensation material, but analyzed according to photoelectric current, TiO2It is higher in the optical absorption intensity of ultraviolet region, but photoelectric current is multiple lower than FLT nanometers
Condensation material, reason may be speed of the light induced electron in conjunction with hole faster, in TiO2With Fe3O4After-LDH load, ABSORPTION EDGE
Edge does not move, and illustrates TiO2With Fe3O4After-LDH load, it can change without band.
Embodiment 3
The present invention is by FLT nanocomposite applications in absorption and photo catalytic reduction research to Cr (VI).
(1) absorption test
Cr (VI) solution of 100mL 20mg/L or 50mg/L and 100mg FLT nanocomposite are placed in 250mL stone
Ying Guanzhong determines the equilibration time that FLT nanocomposite adsorbs Cr (VI) at room temperature by dynamic experiment；Selection stirring
Time is 5min-180min, and separates to obtain supernatant in 8000r/min centrifugation 7min；For adsorption isotherm, by various concentration
Cr (VI) solution be uniformly mixed with 100mg FLT nanocomposite, reach adsorption equilibrium.
(2) photocatalysis is tested
Under ultraviolet light, the photocatalysis performance of FLT nanocomposite is measured by reduction Cr (VI) solution；Three
In a 250mL quartz ampoule, it is separately added into 100mL Cr (VI) solution, then is separately added into FLT-1, FLT-2, FLT-5 of 100mg and receives
Nano composite material is opened the mercury lamp for 4 5W that wavelength is 254nm, magnetic agitation 120min, to ensure Cr (VI) in composite wood
Adsorption-desorption balances on material；After the reaction was completed, certain intervals take out 3mL residual solution, and are centrifugated in 8000r/min
10min measures photocatalysis effect with ultraviolet specrophotometer, evaluates FLT-1, FLT-2, FLT-5 by calculating degradation efficiency
Degradation efficiency is defined as c/c by the photocatalysis effect of nanocomposite0, wherein c0For Cr (VI) initial concentration solution, c is light
Concentration after catalysis irradiation.
(3) measuring method
The measurement of Cr (VI) concentration uses diphenylcarbazide development process, and detection is limited to 0.005mg/L, by above-mentioned centrifugation point
0.45 μm of film is crossed from obtained supernatant liquor, and color developing agent is added, color developing agent includes sulfuric acid solution, phosphoric acid solution and hexichol phosphinylidyne
The colour developing of two hydrazines；When solution colour is stablized, Cr (VI) residual concentration in supernatant is measured in 540nm with spectrophotometer.
(4) adsorption dynamics adsorption kinetics and thermoisopleth research
Adsorption dynamics adsorption kinetics analysis is to remove an importance of pollutant research, and quasi- first-level model and quasi- second-level model are
It predicts the most frequently used model of mechanism involved in adsorption process, intends the linear equation (Eqn. (S1)) of level-one, intend second level linear equation
(Eqn. (S2)) equation may be expressed as:
Q in formulaeAnd qtIt (mg/g) is respectively to be adsorbed on the Cr (VI) on adsorbate with t (min) moment when balancing and measure.k1(1/
) and k min2(g/ (mgmin)) is the rate constant of quasi- level-one and quasi- second order dynamic model, intends second level equation and describes being
Absorption is learned, intending First-order equation description is physical absorption, therefore quasi- level-one and quasi- second level can better describe Cr (VI) and exist
Absorption on LDHs.
It is further using Freundlich equation (Eqn (S3)) and two kinds of balance models of Langmuir equation (Eqn (S4))
It is fitted adsorption isotherm data.
Wherein qe(mg/g) and ceIt (mg/L) is the equilibrium adsorption concentration of solute in solid phase and water phase, qmIt (mg/g) is maximum
Adsorption capacity, k and n are Freundlich constant, related with adsorption capacity and adsorption strength, and b (L/mg) is related to adsorption energy
Langmuir constant.
The reaction time of FLT nanocomposite and Cr (VI) absorption influences as shown in Figure 10 (a), the results showed that, TiO2、
Fe3O4- LDH, FLT-1, FLT-2, FLT-5 nanocomposite reach adsorption equilibrium in 120min, intend first-level model and intend
Shown in the parameter of second-level model such as table 1 and Figure 10 (b), from coefficient R2As can be seen that the data are dynamic more suitable for quasi- second level
Mechanics；This show reaction rate may be by the chemisorption of the shared of the electronics between adsorbate and adsorbent or exchange and
It determines；Fe3O4The equilibrium adsorption ability of-LDH is lower, but in load TiO2Afterwards, FLT-2 even compares Fe3O4- LDH has more preferable
Absorption property, this illustrates TiO2With Fe3O4The combination of-LDH effectively increases adsorption capacity.
Cr (VI) is in Fe3O4When adsorption isotherm on-LDH, FLT-1, FLT-2, FLT-5 nanocomposite is studied, choosing
With adsorbent Fe3O4- LDH, FLT-1, FLT-2, FLT-5 nanocomposite dosage be 0.10g, sorption reaction time is
120min, pH are carried out under conditions of being 3, as a result as shown in Figure 10 (c), Figure 10 (d)；Data are by Freundlich and Langmuir
Isotherm model fitting, model parameter is as shown in table 2, and the equilibrium adsorption ability of each material increases；When Cr (VI) is initial
When concentration increases, mass transfer driving force enhances, Cr (VI) and adsorbent Interaction enhanced, so that adsorption capacity is improved, FLT's
Equilibrium adsorption ability is weaker than Fe3O4- LDH, main cause are the Fe in adsorption process3O4- LDH plays primary attachment, with dense
The increase of degree, Fe3O4The adsorption site of-LDH in the composite is occupied completely, and Cr (VI) is in Fe3O4Adsorbance on-LDH
It is relatively high, but Fe3O4- LDH and TiO2The combination of two kinds of materials promotes absorption, therefore FLT and Fe3O4The difference of-LDH compared with
It is small.As shown in Table 2, the coefficient R of Langmuir equation2Greater than Freundlich equation, illustrate that adsorption process more meets
Langmuir equation.
1 Fe of table3O4The kinetic parameter that-LDH and FLT composite material adsorb Cr (VI)
2 Fe of table3O4The adsorption isotherm parameter of-LDH and FLT composite material to Cr (VI)
(5) photocatalytic activity
In order to test the photocatalysis performance of FLT nanocomposite that the present invention is prepared, it is based on the above absorption result,
It selects Cr (VI) as target contaminant, studies Cr (VI) photo catalytic reduction under ultraviolet light and test, as a result as shown in Figure 11 (a),
The rate of reduction that pollutant is described using first order rate constant is calculated using first order reaction model:
-ln(c/c0)=kt
Wherein c0Cr (VI) concentration and in Cr (VI) concentration of illumination t min when being respectively balance after illumination with c.
TiO2、Fe3O4- LDH, FLT-1, FLT-2, FLT-5 nanocomposite react speed to the photo catalytic reduction of Cr (VI)
Shown in rate result such as Figure 11 (b), You Tuzhong the result shows that, FLT-2 sample is better than other materials to the catalytic performance of Cr (VI),
The rate constant ratio Fe of FLT-23O4- LDH is 3.7 times high, compares TiO2It is 28 times high；This is because there is semiconductor in the composite
TiO2Presence, free electron and hole can be provided under ultraviolet light for redox reaction；Work as TiO2Ratio very little when,
It may be due to caused by the activated centre deficiency of material offer that photocatalytic activity, which reduces,；But with TiO2The increase of ratio, it is compound
The effect of material is also deteriorated, and reason may be TiO2Reunion and Fe3O4- LDH and TiO2In conjunction with reduction cause photocatalysis living
The reduction of property；In conjunction with the above results, TiO2The FLT-2 that content is 20% has optimal photocatalytic activity, mainly has benefited from it
Good absorption and photocatalysis performance, work as TiO2Content be 20% when, FLT nanocomposite adsorption site with higher and
Good electric charge transfer performance, Fe3O4- LDH and 20%TiO2When two kinds of Material claddings, light induced electron and sky can be inhibited significantly
The recombination in cave improves the photocatalytic activity of product.
(6) absorption and photo-reduction performance of FLT-2
The removal rate of Cr (VI) is the FLT nanocomposite of evaluation preparation, TiO2And Fe3O4The absorption of-LDH material and
A kind of method of photo catalytic reduction ability；As shown in Figure 12 (a), Figure 12 (b), respectively FLT nanocomposite, TiO2And
Fe3O4The effect of the removal of-LDH material 20mg/L Cr (VI) and 50mg/L Cr (VI)；As can be seen that removing TiO from Figure 12 (b)2
Outside, all material is attained by good removal effect；Wherein Fe3O4The adsorption effect of-LDH is best, nano combined better than FLT
Material and TiO2, reason may be Fe3O4- LDH has more adsorption sites than FLT nanocomposite；In ultraviolet lighting
It penetrates down, different materials can reach very high removal rate in a short period of time；But the 50mg/L shown in Figure 12 (a)
In Cr (VI) solution, FLT-2 almost 100% removal Cr (VI) from solution, FLT-1, FLT-5 distinguish the removal rate of Cr (VI)
For 87.93%, 82.61%, Fe3O4The removal rate of-LDH is 75.87%；To sum up, the eliminating rate of absorption highest of FLT-2,
Secondary is Fe3O4- LDH, FLT-1 are finally FLT-5, the reason is that mass transfer driving force becomes strong, and TiO2The lower FLT-2 of content is to Cr
(VI) removal rate most preferably mainly has benefited from its good absorption and photocatalysis performance.
Table 3 compares in the present invention in FLT nanocomposite and other researchs catalyst to Cr (VI) concentration removal rate
Comparative result, by table 3, the result shows that, FLT-2 nanocomposite of the present invention is apparently higher than other to the removal rate of Cr (VI)
Research, FLT-2 nanocomposite of the present invention are applicable not only to the processing of low concentration wastewater, are also applied for the place of high-concentration waste water
Reason；And TiO is used alone2It is undesirable to the treatment effect of two kinds of concentration waste water.Therefore, composite material can give full play to often
A kind of the advantages of list material.
3 different catalysts of table compare Cr (VI) solution synergy of various concentration
Embodiment 4
In order to evaluate the stability and recycling property of catalyst of the present invention, using one-step method to FLT-2 nanocomposite
Material after absorption Cr (VI) is regenerated, and being handled by 0.5mol/L NaOH restores its adsorption site；By the recovery of recycling
The FLT-2 nanocomposite of adsorption site carries out 5 recyclings, and removal contains the waste water of 50mg/LCr (VI), as a result as schemed
Shown in 13；In first circulation, 63.46% Cr (VI) is eliminated, but tend towards stability after the 4th circulation, Adsorption
Rate is about 43.10%, under the conditions of synergistic sorption and photocatalysis, the eliminating rate of absorption difference of first circulation and the 5th circulation
About 25%；Reason may be that photo catalytic reduction product Cr (III) covers surface-active site, when the nano combined material of FLT-2
After material is reused, Cr (III) content of adsorption is gradually increased, and influences photocatalysis performance；As shown in Figure 13, at the 5th time
In use, FLT-2 remains to reach 40% to the removal rate of Cr in waste water (VI), this illustrates that FLT composite material of the invention has
Preferable reusing.
Embodiment 5
The mechanism of Cr (VI) ion in water removal is gone to be studied FLT:
The mechanism that LDHs adsorbs heavy metal ion includes precipitating, surface complexing, isomorphism substitution and chelating, is as shown in figure 14
The infrared analysis map of FLT, AFLT-2, RFLT-2, wherein AFLT-2 is that FLT-2 nanocomposite adsorbs the material after Cr (VI)
Material；RFLT-2 is material after Cr (VI) catalysis reduction；As shown in Figure 14, FLT-2, AFLT-2 and RFLT-2 are in 581cm-1With
910cm-1Peak strength difference illustrate that Cr (VI) reacts with M-O, Fe-O, the variation of OH and M-OH are since Cr (VI) is molten
Caused by the property of liquid.
In XPS, the transfer of the content, the combination energy of element of element in peak strength expression material, and combine the increasing of energy
Add be due to caused by the reduction of electron density, LDHs absorption heavy metal ion mechanism can also be obtained by XPS analysis
To confirmation；The peak of Cr 2p3/2 and Cr 2p1/2 when combination can be respectively 579.3 and 586.4eV in Figure 15 (b) is very close
K2Cr2O7The peak of middle Cr 2p, this shows that Cr (VI) and FLT-2 are physical bonds, and pH value is lower, photocatalyst surface cation number
Increase, to promote Cr2O7 2-,HCrO4 -And CrO4 2-Electrostatic attraction；When the pH of solution is 1.0-7.0, Cr (VI) is main
Existence form is Cr2O7 2-And HCrO4-, when the solution ph of anion is higher than 7.0, Cr (VI) is predominantly in the form of
CrO4 2-；The peak value meter of 577.6eV is bright to generate new key Zn-Cr-O and Fe-Cr-O, thus illustrate material and Cr (VI) it
Between absorption be chemisorption；The peak value of photo catalytic reduction Cr (VI) material afterwards is in 586.9eV, 579.1eV, 577.1eV, respectively
For Cr 2p 3/2 and Cr 2p 1/2, it was demonstrated that Cr (VI) has been reduced into Cr (III), also thus illustrates that this is that an oxidation is gone back
Original reaction；It can be seen that the displacement between the material after FLT-2 material is reacted with Cr (VI) from Figure 15 (a) and show that Fe takes part in
Cr (VI) reaction, and in combination form novel substance；But the peak no significant difference of AFLT-2 and RFLT-2, reason may be Fe
It is not engaged in redox reaction；Shown in O 1s XPS spectrum figure such as Figure 15 (c), the peak of FLT-2 is at 528.3eV and 530.5eV points
Ti-O, M-O are not corresponded to, illustrate material absorption Cr (VI) in 529.9eV and 531.7eV and forms Cr (VI) with O in lattice
New species CrO3；Peak turns to 530.1eV from 529.9eV, and the transformation at peak means electronics from nano-titanium dioxide surface a part
It is transferred to FLT-2 material surface and forms Cr2O3；Shown in spectrum such as Figure 15 (d) of the Ti 2p 1/2 and Ti 2p 3/2 of sample,
TiO2Middle 3/2 peak Ti 2p is transferred to 458.2eV from 456.9eV, by adsorbing and Ti in FLT-2 material after photocatalytic process
1/2 peak 2p is transferred to 464.1eV, this sharp deflections explanation from 462.6eV, and the chemical environment of Ti has apparent difference, nanometer
TiO2Adjacent difference between Ti 2p 1/2 and Ti 2p 3/2 is that 5.8eV is identical as FLT-2 composite material, illustrates TiO2?
Grain is in Fe3O4The sharpening structure still coordinated with octahedral on-LDH.
By in tem analysis it will be clear that Fe3O4And TiO2It is attached to the surface Zn-Al-LDH, is effectively promoted
The reduction of Cr (VI), while according to catalysis characterization result, it can rationally infer that there is FLT-2 good photocatalytic activity mainly to obtain
Beneficial to its excellent absorption property and electric charge transfer performance, FLT-2 has apparent synergistic effect between absorption and photocatalysis；
It analyzes by photoelectric current it is found that FL composite material and TiO2Form hetero-junctions, it is suppressed that photoelectron and hole-recombination are conducive to promote
Into the photocatalytic activity of product.
In conclusion passing through TiO2And Fe3O4- LDH sol-gel method successfully synthesizes FLT composite material, passes through absorption
Remove Cr (VI) with photocatalysis synergy, and a series of phenetic analysis carried out to the structure of FLT-2, from XRD, XPS and
FTIR spectrogram can be seen that the FLT-2 being prepared by Fe3O4, Zn-Al-LDH and TiO2Phase composition, and sample purity is higher；
By the spherical Fe of SEM, TEM and HRTEM display3O4With columnar TiO2It is attached to the surface stratiform Zn-Al-LDH, and in FLT-2
Fe3O4、FL、TiO2Lattice fringe between be divided into 0.2943nm, 0.3507nm, 0.2774nm, quite connect with the XRD spacing of FLT-2
Closely；By photoelectric current and electrochemical impedance, the result shows that, the formation of hetero-junctions inhibits photoelectron and hole recombination, therefore, FL and
TiO2Between synergistic effect enhancing, obtained FLT-2 nano composite material photocatalyst removal Cr (VI) in terms of performance
Biggish photocatalytic activity out, the rate constant of FLT-2 are 3.7 times and TiO of FL respectively228 times, and to containing 20mg/
L, 50mg/L Cr (VI) water treatment effect is good, illustrates that FLT-2 is applicable not only to low concentration wastewater processing, is also applied for height
Concentration wastewater treatment.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes
It also should be regarded as protection scope of the present invention into supplement；All those skilled in the art, do not depart from spirit of that invention and
In the case where range, using the equivalent variations of a little change, modification and differentiation that disclosed above technology contents are made, it is
Equivalent embodiment of the invention；Meanwhile any equivalent variations that all substantial technologicals according to the present invention do above-described embodiment
Change, modification and differentiation, still fall within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material, which comprises the steps of:
The preparation of S1, magnetic hydrotalcite: Zn (NO will be contained3)2.6H2O、Al(NO3)3.9H2The mixed salt solution of O and contain
NaOH、Na2CO3Mixed ammonium/alkali solutions be added drop-wise to Fe3O4Water slurry solution in carry out coprecipitation reaction, be centrifuged, collect solid phase
Object cleans solid formation to neutrality with deionized water, dries to get magnetic hydrotalcite is arrived；
The preparation of S2, magnetic hydrotalcite carried titanium dioxide composite material: by TiO2It is distributed in PEG (200), step S1 is added
Magnetic hydrotalcite obtained, TiO2Mass ratio with magnetic hydrotalcite is 1:1-10, and ultrasonic 20-40min obtains slurries；
S3, above-mentioned slurries are subjected to hydrothermal crystallizing processing, after the reaction was completed, solid formation is collected in centrifugation, is cleaned with deionized water solid
Phase object, it is dry, obtain magnetic hydrotalcite carried titanium dioxide composite material.
2. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 1, feature
It is, Fe is pressed in step S13O4And Al3+Molar ratio is (0.1~1): 1 ratio weighs Fe3O4, in stirring and 60 DEG C of water-bath items
Under part, Zn (NO will be contained3)2.6H2O、Al(NO3)3.9H2The mixed salt solution of O and contain NaOH, Na2CO3Mixed base
Solution is added drop-wise to Fe3O4Water slurry solution in, and adjust reaction system pH value be 9~10, carry out coprecipitation reaction.
3. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 2, feature
It is, weighs Zn (NO according to the ratio that zinc-aluminium molar ratio is 2: 1 in step S13)2.6H2O、Al(NO3)3.9H2O。
4. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 2, feature
It is, weighs Na according to the ratio that mass ratio is 9: 7 in step S12CO3With NaOH.
5. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 1, feature
It is, drying temperature is 40-60 DEG C in step S1.
6. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 1, feature
It is, further includes that the magnetic hydrotalcite that will be obtained sieves with 100 mesh sieve in step S1.
7. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 1, feature
It is, in step S3, the temperature of hydrothermal crystallizing processing is 80-100 DEG C, time 1-2h.
8. a kind of preparation method of magnetic hydrotalcite carried titanium dioxide composite material according to claim 1, feature
It is, in step S3, drying temperature is 60 DEG C.
9. magnetic hydrotalcite carried titanium dioxide composite material made from preparation method according to any one of claims 1 to 8
Application in processing water in Cr (VI).
10. application according to claim 9, which is characterized in that the application is the following steps are included: by the magnetic neatly
Stone carried titanium dioxide composite material is mixed with containing Cr (VI) waste water, reaches adsorption equilibrium, is opened ultraviolet lamp progress light and is urged
Change reduction, completes the processing to Cr (VI) waste water is contained.
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